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DC magnetization of titania supported on reduced graphene oxide flakes

  • Niko Guskos , Grzegorz Zolnierkiewicz EMAIL logo , Aleksander Guskos , Konstantinos Aidinis , Spiros Glenis , Agnieszka Wanag , Ewelina Kusiak-Nejman , Urszula Narkiewicz and Antoni W. Morawski
Published/Copyright: October 19, 2021
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REVIEWS ON ADVANCED MATERIALS SCIENCE
From the journal REVIEWS ON ADVANCED MATERIALS SCIENCE Volume 60 Issue 1

Abstract

DC magnetization of a series of titania nanocomposites modified with reduced graphene oxide (rGO) has been investigated. Hysteresis loops observed at room temperature disappeared at low temperatures. At a temperature of about 100 K, a phase transition to the superferromagnetic order state was observed, probably due to the linear expansion and self-reorientation of the magnetic moments. Processes associated with magnetic moment reorientation can cause a hysteresis loop to disappear at low temperatures as well as superferromagnetic ordering. It was suggested that the isolated nanoparticle in the nanopore could be used to create a “compass” at a nanometer-sized level that would be many times more sensitive than the conventional one. Measurements of the zero-field cooling and field cooling modes do not exclude the possibility of the coexistence of a superparamagnetic state.

Keywords: magnetism; nanocomposites TiO2/rGO; phase transition

1 Introduction

A semiconducting material, TiO2−δ with ferromagnetism up to 880 K, without the introduction of magnetic ions were obtained [1]. They can be also applied to spintronics devices. According to the calculations, a stable ferromagnetic ground state [2] can occur in Cr-doped rutile TiO2. Enhanced ferromagnetic properties were observed in N-doped TiO2 [3]. The saturation magnetization at room temperature was in the order of Fe + N doped TiO2 > N-doped TiO2 ≫ Fe-doped TiO2 > undoped TiO2.

Density functional theory calculations were done for copper-doped titania (anatase and rutile) [4]. Ferromagnetism is predicted to be stable well above the room temperature with long-range interactions prevailing in the anatase phase and short-range interactions in the rutile phase.

Choudhury and Choudhury [5] investigated room temperature ferromagnetism exhibited by nonmagnetic metal oxide semiconductor nanostructures, considering an example of air and vacuum annealed titania nanoparticles. According to the obtained results, ferromagnetism is a nanoscale surface phenomenon in titania NPs, correlated with the presence of paramagnetic Ti3+ and F+ (oxygen vacancies) centers.

Ferromagnetic ordering at room temperature has been induced in the rutile phase of the TiO2 polycrystalline sample by O ion irradiation [6]. The structural, electronic and magnetic properties of intrinsic defects in anatase-type ultrathin TiO2 nanotubes have been investigated systematically by first-principles calculations [7]. This work offers a possible route toward high Curie temperature ferromagnetism in TiO2 materials. Undoped and Ni-doped TiO2 (xNi = 0.00, 0.50, 1.00, 1.50, 2.00 and 2.50 wt%) at room-temperature ferromagnetism has been investigated [8]. The addition of Ni did not affect the crystallinity of the samples but influenced the ferromagnetic behavior, which allows for potential spintronic applications of Ni-doped TiO2 diluted magnetic semiconductors.

Recently, a new generation of nanocomposites for electronic circuit applications has appeared, based on titania modified with rGO [9,10,11,12,13]. Scientists dealing with these nanocomposites approve the importance of dynamic and static magnetic interactions by localized magnetic centers and the formation of magnetic aggregates (clusters) magnetic in physical processes. The most effective methods to study these phenomena are EPR/FMR (electron paramagnetic resonance)/(ferromagnetic resonance) and DC magnetization measurements by SQUID.

In our previous paper [14], EPR/FMR measurements of the whole series of titania nanocomposites modified with reduced graphene oxide (rGO) were reported. A ferromagnetic ordering and localized magnetic moments originating from oxygen defects in nanocomposite particles as well as from free radicals and trivalent titanium ions were observed, and their number depended on the calcination temperature. The application of appropriate proportions of these species improved the photocatalytic properties of the nanocomposites. The aim of the present work is to continue the previous studies [14] of magnetic properties by supplementary and in-depth investigation through the DC magnetization method (the same series of samples). Depending on calcination temperature, we can observe magnetic phase transitions, superparamagnetic state or the appearance of the hysteresis loop.

2 Experimental

Preparation of the titania-based nanocomposites modified with reduced graphene oxide (rGO) and their characteristics were previously described [14]. In the previous work, an attempt to correlate the magnetic properties of the titania/rGO nanocomposites with their photocatalytic activity has been made.

DC magnetization measurements were carried out using an MPMS-7 SQUID magnetometer in a 2–300 K temperature range and under a magnetic field up to 70 kOe, both in the zero-field cooling (ZFC) and field cooling (FC) modes.

3 Results and discussion

Figure 1 shows the temperature dependence of DC magnetic susceptibility χ(T) (here, χ is defined as χ = M/H, where M is the magnetization and H an external magnetic field) and the reciprocal magnetic susceptibility χ – 1(T) of the nanocomposites TiO2/rGO-8-400, TiO2/rGO-8-500 and TiO2/rGO-8-600 in the ZFC mode. The samples under study were registered in an external different magnetic field H in ZFC (zero-field cooling) and FC (field cooling) modes. The nanocomposite TiO2/rGO-8-400 under a low applied external magnetic field showed the highest magnetic susceptibility (Figure 1). For higher values of the applied external magnetic field, the obtained dependencies were similar to those for other samples.

Figure 1 Temperature dependence of magnetic susceptibility and its inverse, ZFC mode.
Figure 1

Temperature dependence of magnetic susceptibility and its inverse, ZFC mode.

At the nano and macro levels, the magnetic moments are subject to the laws of classical physics. There is a well-known case of two compasses: when we bring them closer to an appropriate distance (depending on the magnetization of the needles), they positioned themselves anti-parallelly, while by applying an external magnetic field of appropriate intensity, they can line up parallelly. By applying magnetic nanoparticles in a small concentration, we can obtain a superparamagnetic state and there is a strong dependence of magnetic susceptibility in ZFC and FC modes [15,16]. Magnetic susceptibility decreases with increased calcination temperatures in the ZFC modes at low values of the transferred magnetic fields and, in both cases, at higher fields, this process disappears. We can note that GO and rGO DC measurements of magnetization showed a strong paramagnetic relationship [16]. When modifying titanium dioxide with rGOs, a resulting magnetic state is diametrically more complex. In all investigated nanocomposites, hysteresis loops were observed at room temperature (Figure 2) and disappeared at lower temperatures. At temperature 2 K, we can see in Figure 2 that remanent magnetization and coercive field are almost equal to zero so we can state that there is no hysteresis loop at 2 K. Table 1 lists the parameters describing the hysteresis loops at room temperature. So, we can assume that we have sparse “compasses” in the studied nanocomposites.

Figure 2 Dependence of magnetization on the magnetic field at T = 2 K and room temperature.
Figure 2

Dependence of magnetization on the magnetic field at T = 2 K and room temperature.

Table 1

Parameters of the magnetic hysteresis loop at room temperature

TiO2/rGO-8-400 TiO2/rGO-8-500 TiO2/rGO-8-600
Hc (Oe) Mr (emu·g−1) Hc (Oe) Mr (emu·g−1) Hc (Oe) Mr (emu·g−1)
60 5.3 × 10−4 50 7.7 × 10−5 106 7.7 × 10−5

When high magnetic fields are applied to nanocomposites TiO2/rGO-8-400 and TiO2/rGO-8-600, a diamagnetism dominates at room temperature (Figure 2). In the case of nanocomposite TiO2/rGO-8-500, we have a greater amount of trivalent titanium ions [14] and hence the behavior of magnetization is opposite. Some differences in reaching the diamagnetic state may be due to the different concentrations of localized magnetic moments. In all nanocomposites, paramagnetic behavior at low temperatures is dominant, and hence, we have a similar magnetization behavior under the influence of the applied magnetic field.

Figure 3 shows the dependence of inverse magnetic susceptibility on temperature for a nanocomposite TiO2/rGO-8-400 in ZFC and FC modes at an applied magnetic field H = 100 Oe. There is a significant difference in inverse magnetic susceptibility at lower values of the applied magnetic field. This is due to the possibility of setting some anti-parallel magnetic moments. Below 100 K, we can observe a transition of magnetic moment systems from anti-parallel to ferromagnetic order, where below 50 K, there is an almost “paramagnetic” state. For a field 1,000 Oe in the FC mode (for all samples) after a linear extension of the 1/χ curve below about 100 K, the extension crosses the positive coordinate of the temperature axis; therefore, we conclude that there is a superferromagnetic order of magnetic moments. Magnetic nanoparticles are smaller in size than the nanopores and hence they are more mobile and the resulting internal magnetic field can act in order. With high values of the intensity of the external magnetic field, the transition to the ferromagnetic state takes place at about 100 K. In the case of nanocomposites TiO2/rGO-8-500 and TiO2/rGO-8-600, the transition occurred at about 90–100 K. The lower value of the critical temperature for the nanocomposite TiO2/rGO-8-500 may be related to the presence of a greater amount of trivalent titanium ions [14].

Figure 3 Temperature dependence of inverse magnetic susceptibility in ZFC and FC modes for the nanocomposite TiO2/rGO-8-400 at an applied magnetic field H = 100 Oe.
Figure 3

Temperature dependence of inverse magnetic susceptibility in ZFC and FC modes for the nanocomposite TiO2/rGO-8-400 at an applied magnetic field H = 100 Oe.

Table 2 shows the values of the magnetic susceptibility at room temperature and at T = 2 K. At a temperature of T = 2 K, the magnetic susceptibility decreased with increasing calcination temperature for small external magnetic fields. By increasing the intensity of the applied external magnetic field, the magnetic susceptibility decreased. In the case of the TiO2/rGO-8-400 nanocomposite, the greatest difference in magnetic susceptibility in FC and ZFC modes was noticed (Figure 3). Probably, some of the magnetic moments aligned anti-parallely under the influence of the magnetic field. At room temperature, the lowest magnetic susceptibility value was obtained for the nanocomposite TiO2/rGO-8-600. The highest value was obtained for the nanocomposite TiO2/rGO-8-400 after applying a low external magnetic field. These results confirm that the smallest number of magnetic moments was found in the nanocomposite TiO2/rGO-8-600, where the photocatalytic efficiency was the highest [14].

Table 2

Magnetic susceptibility at temperatures of 2 and 300 K

T = 2 K
H (Oe) TiO2/rGO-8-400 TiO2/rGO-8-500 TiO2/rGO-8-600
ZFC FC ZFC FC ZFC FC
(10−5 emu·(g·Oe)−1)
10 3.9 4.9 1.8 1.9 0.9 0.9
100 1.7 2.0 1.9 2.0 0.8 0.9
1,000 1.7 1.9 2.1 2.1 0.9 1.0
70,000 0.9 1.0 1.0 1.0 0.5 0.5
T = 300 K
H (Oe) TiO2/rGO-8-400 TiO2/rGO-8-500 TiO2/rGO-8-600
ZFC FC ZFC FC ZFC FC
(emu·(g·Oe)−1)
10 2.4 × 10−5 4.1 × 10−5 3.6 × 10−6 3.3 × 10−6 2.3 × 10−6 2.3 × 10−6
100 8.7 × 10−6 8.9 × 10−6 2.1 × 10−6 2.1 × 10−6 7.9 × 10−7 8.1 × 10−7
1,000 3.8 × 10−6 3.4 × 10−6 1.8 × 10−6 1.8 × 10−6 5.2 × 10−7 5.3 × 10−7
70,000 −2.7 × 10−7 −2.6 × 10−7 2.8 × 10−7 2.8 × 10−7 −1.8 × 10−7 −1.8 × 10−7

At very low temperatures, a magnetic susceptibility to oxygen defects related to trivalent titanium ions and free radicals was observed, which at low values of the external magnetic fields were subjected to the Curie-Weiss law with a negative Curie-Weiss temperature value. With higher applied external magnetic fields, the susceptibility followed the Curie law, probably due to the anti-parallel setting of magnetic moments associated with trivalent titanium ions [14].

At lower temperatures, the resonance lines of magnetic nanoparticles significantly shifted, increasing the internal magnetic field [17,18]. In the papers [19,20], a very small occurrence of magnetic clusters in nitrogen-reduced titanium dioxide was determined using the FMR method. In collaboration with the chemical engineering research group, a concept was developed to create a material based on the modified titanium dioxide, an ordering system of magnetic moments, created by the action of the internal magnetic field (superferromagnetic state). As a result of the effect of thermal expansion, a large internal magnetic field was generated at a certain temperature. The generated internal magnetic field affects the magnetic domains that cancel hysteresis loops at lower temperatures.

The materials under study are porous, and hence, we can consider the placement of magnetic moments in the pores as “compasses” at the nano level. By tuning the nanoparticles’ size and porosity, we can create in the future a much more sensitive “compass” system.

The observed super-ferromagnetic state occurs significantly above the temperature of liquid nitrogen, which would be important because of the lower cost of future electromagnetic devices. In our previous work, we also showed that such a state was favorable for photocatalytic properties [14]. Since the magnetic ordering is dominated by trivalent titanium ions, creating magnetic hysteresis can influence the photocatalytic processes.

Since the magnetic ordering and the accompanying magnetic hysteresis are related to the trivalent titanium ions, the formation of hysteresis loops has a complex character. Because it is associated with titanium ions at a lower oxidation rate, it causes the disappearance of the hysteresis loop at lower temperatures, for example, due to the change in thermal expansion.

The hysteresis loop disappeared at low temperature; nevertheless, it is not possible to verify if this phenomenon could affect photocatalytic activity, as the photocatalytic process is carried out in water at room (or higher) temperature. The disappearance of the hysteresis loop at low temperatures may be due to the processes of reorientation of magnetic moments.

4 Conclusion

Measurements of the temperature dependence of DC magnetization in the ZFC and FC modes of a series of nanocomposites modified with reduced graphene oxide (rGO) were performed. The conclusions drawn in the previous work on magnetic resonance investigation [14] were confirmed. At room temperature, magnetic hysteresis was observed in all investigated nanocomposites, which disappeared at low temperatures. It is probably related to change of the internal magnetic field due to reorientation of spin systems. In the modified titanium dioxide, a superferromagnetic state was obtained by ordering magnetic moments through the resulting internal magnetic field.

Acknowledgements

The research leading to these results has received funding from the Norway Grants 2014-2021 via the National Centre for Research and Development under the grant number NOR/POLNORCCS/PhotoRed/0007/2019-00.

  1. Funding information: The research leading to these results has received funding from the Norway Grants 2014-2021 via the National Centre for Research and Development under the grant number NOR/POLNORCCS/PhotoRed/0007/2019-00.

  2. Author contributions: Conceptualization: NG; data curation: GZ, KA, and SG; formal analysis: GZ; funding acquisition: UN; methodology: NG, UN, EKN, and AWM; investigation: GZ, AG, and AW; project administration: NG, UN, and AWM; resources: GZ., EKN, AG, and KA; software: GZ, AG, and KA; supervision: NG, and AWM; validation: NG, GZ, UN, AWM; visualization: GZ, KA; writing – original draft: NG, and UN; writing – review & editing: NG, GZ, UN, and EKN. All authors have read and agreed to the published version of the manuscript.

  3. Conflict of interest: The authors declare no conflict of interest. The funders had no role in the design of the study; in the collection, analyses, or interpretation of data; in the writing of the manuscript, or in the decision to publish the results.

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Received: 2021-04-24
Revised: 2021-06-15
Accepted: 2021-08-19
Published Online: 2021-10-19

© 2021 Niko Guskos et al., published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

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https://doi.org/10.1515/rams-2021-0059
Keywords for this article
magnetism; nanocomposites TiO2/rGO; phase transition
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  15. Revealing grain coarsening and detwinning in bimodal Cu under tension
  16. Mesoporous silica nanoparticles functionalized with folic acid for targeted release Cis-Pt to glioblastoma cells
  17. Magnetic behavior of Fe-doped of multicomponent bismuth niobate pyrochlore
  18. Study of surfaces, produced with the use of granite and titanium, for applications with solar thermal collectors
  19. Magnetic moment centers in titanium dioxide photocatalysts loaded on reduced graphene oxide flakes
  20. Mechanical model and contact properties of double row slewing ball bearing for wind turbine
  21. Sandwich panel with in-plane honeycombs in different Poisson's ratio under low to medium impact loads
  22. Effects of load types and critical molar ratios on strength properties and geopolymerization mechanism
  23. Nanoparticles in enhancing microwave imaging and microwave Hyperthermia effect for liver cancer treatment
  24. FEM micromechanical modeling of nanocomposites with carbon nanotubes
  25. Effect of fiber breakage position on the mechanical performance of unidirectional carbon fiber/epoxy composites
  26. Removal of cadmium and lead from aqueous solutions using iron phosphate-modified pollen microspheres as adsorbents
  27. Load identification and fatigue evaluation via wind-induced attitude decoupling of railway catenary
  28. Residual compression property and response of honeycomb sandwich structures subjected to single and repeated quasi-static indentation
  29. Experimental and modeling investigations of the behaviors of syntactic foam sandwich panels with lattice webs under crushing loads
  30. Effect of storage time and temperature on dissolved state of cellulose in TBAH-based solvents and mechanical property of regenerated films
  31. Thermal analysis of postcured aramid fiber/epoxy composites
  32. The energy absorption behavior of novel composite sandwich structures reinforced with trapezoidal latticed webs
  33. Experimental study on square hollow stainless steel tube trusses with three joint types and different brace widths under vertical loads
  34. Thermally stimulated artificial muscles: Bio-inspired approach to reduce thermal deformation of ball screws based on inner-embedded CFRP
  35. Abnormal structure and properties of copper–silver bar billet by cold casting
  36. Dynamic characteristics of tailings dam with geotextile tubes under seismic load
  37. Study on impact resistance of composite rocket launcher
  38. Effects of TVSR process on the dimensional stability and residual stress of 7075 aluminum alloy parts
  39. Dynamics of a rotating hollow FGM beam in the temperature field
  40. Development and characterization of bioglass incorporated plasma electrolytic oxidation layer on titanium substrate for biomedical application
  41. Effect of laser-assisted ultrasonic vibration dressing parameters of a cubic boron nitride grinding wheel on grinding force, surface quality, and particle morphology
  42. Vibration characteristics analysis of composite floating rafts for marine structure based on modal superposition theory
  43. Trajectory planning of the nursing robot based on the center of gravity for aluminum alloy structure
  44. Effect of scan speed on grain and microstructural morphology for laser additive manufacturing of 304 stainless steel
  45. Influence of coupling effects on analytical solutions of functionally graded (FG) spherical shells of revolution
  46. Improving the precision of micro-EDM for blind holes in titanium alloy by fixed reference axial compensation
  47. Electrolytic production and characterization of nickel–rhenium alloy coatings
  48. DC magnetization of titania supported on reduced graphene oxide flakes
  49. Analytical bond behavior of cold drawn SMA crimped fibers considering embedded length and fiber wave depth
  50. Structural and hydrogen storage characterization of nanocrystalline magnesium synthesized by ECAP and catalyzed by different nanotube additives
  51. Mechanical property of octahedron Ti6Al4V fabricated by selective laser melting
  52. Physical analysis of TiO2 and bentonite nanocomposite as adsorbent materials
  53. The optimization of friction disc gear-shaping process aiming at residual stress and machining deformation
  54. Optimization of EI961 steel spheroidization process for subsequent use in additive manufacturing: Effect of plasma treatment on the properties of EI961 powder
  55. Effect of ultrasonic field on the microstructure and mechanical properties of sand-casting AlSi7Mg0.3 alloy
  56. Influence of different material parameters on nonlinear vibration of the cylindrical skeleton supported prestressed fabric composite membrane
  57. Investigations of polyamide nano-composites containing bentonite and organo-modified clays: Mechanical, thermal, structural and processing performances
  58. Conductive thermoplastic vulcanizates based on carbon black-filled bromo-isobutylene-isoprene rubber (BIIR)/polypropylene (PP)
  59. Effect of bonding time on the microstructure and mechanical properties of graphite/Cu-bonded joints
  60. Study on underwater vibro-acoustic characteristics of carbon/glass hybrid composite laminates
  61. A numerical study on the low-velocity impact behavior of the Twaron® fabric subjected to oblique impact
  62. Erratum
  63. Erratum to “Effect of PVA fiber on mechanical properties of fly ash-based geopolymer concrete”
  64. Topical Issue on Advances in Infrastructure or Construction Materials – Recycled Materials, Wood, and Concrete
  65. Structural performance of textile reinforced concrete sandwich panels under axial and transverse load
  66. An overview of bond behavior of recycled coarse aggregate concrete with steel bar
  67. Development of an innovative composite sandwich matting with GFRP facesheets and wood core
  68. Relationship between percolation mechanism and pore characteristics of recycled permeable bricks based on X-ray computed tomography
  69. Feasibility study of cement-stabilized materials using 100% mixed recycled aggregates from perspectives of mechanical properties and microstructure
  70. Effect of PVA fiber on mechanical properties of fly ash-based geopolymer concrete
  71. Research on nano-concrete-filled steel tubular columns with end plates after lateral impact
  72. Dynamic analysis of multilayer-reinforced concrete frame structures based on NewMark-β method
  73. Experimental study on mechanical properties and microstructures of steel fiber-reinforced fly ash-metakaolin geopolymer-recycled concrete
  74. Fractal characteristic of recycled aggregate and its influence on physical property of recycled aggregate concrete
  75. Properties of wood-based composites manufactured from densified beech wood in viscoelastic and plastic region of the force-deflection diagram (FDD)
  76. Durability of geopolymers and geopolymer concretes: A review
  77. Research progress on mechanical properties of geopolymer recycled aggregate concrete
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